MEASUREMENT 7. Pumping Speed 5. Pressure Gauges 5.1 Direct –Reading Gauges 5.2 Indirect –Reading Gauges 6. Flow Meters 6.1 Molar Flow, Mass Flow, and Throughput 6.2 Rotameters and Chokes 6.3 Differential Pressure Techniques 6.4 Thermal Mass Flow Meter Techniques 7.1 Pumping Speed 7.2 Mechanical Pumps 7.3 High Vacuum Pumps 8. Residual Gas Analyzer 8.1 Instrument Description 8.2 Installation and Operation 8.3 RGA Calibration 8.4 RGA Selection 9.Interpretation of RGA Data 9.1 Cracking Patterns 9.2 QualitatieAnalysis 9.3 Quantitative Analysis Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung Chapter 5 Pressure Gauges Direct gauge: By calculating the force exerted on the surface by incident particle flux. Indirect gauge: By measuring a gas property that changes in a predictable manner with gas density. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 3.3 Pressure Measurement 3.3.1 Mechanical Gauges –Liquid walls, direct gauge Mercury and oil manometer ** Hg manometer useful down to 1 torr. ** Oil manometer useful down to 0.1 torr. ** Avoid the capillary effect by oil. ** Remove gases inside oil. ** Avoid chemical reaction of Hg with gases by floating a few drops of silicone oil on top of the Hg column. ** Vapor pressure of Hg and oil can be removed by placing a cold trap. Note: Are you measuring a relative or absolute pressure? Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung Hg at 20°C Density = 13.54562 g/cm3 Pvapor = 0.0012 mmHg 3.3.1 Mechanical Gauges –Liquid walls, direct gauge McLeod Gauge: P1V1 = P2V2 = (ρgh)σh P1 = ρσgh2/ V1 ** A sample of gas is trapped and compressed by a known amount (~ 1: 1000). ** The pressure of the compressed gas is measured with a mercury manometer, while the original pressure is determined by the gas law. ** This method is not applicable to a gas that condenses upon compression. ** The McLeod gauge is limited by geometrical constraints to about four orders of magnitude in pressure. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.1. DIRECT-READING GAUGES 5.1.1 Diaphragm and Bourdon Metallic diaphragm gauge - Rough indication of pressure ** The volume on one side of the diaphragm is sealed. ** The volume on the other side is attached to the system. ** A variation in pressure on one side relative to the other causes the diaphragm to flex. -- The precision of both solid-walls gauges are limited by hysteresis caused by friction in the linkage. Tap the gauge before use. -- The solid-walls gauges are not absolute, they have to be calibrated against an absolute gauge (i. e. McLeod) Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.1.1 Diaphragm and Bourdon Bourdon gauge Rough indication of pressure ** A thin-walled metal tube, somewhat flattened and bent into the form of a C. ** Attached to its free end is a lever system that magnifies any motion of the free end of the tube. ** On the fixed end of the gauge is a fitting to the measured system. ** As pressure increases within the measured system, it travels through the tube. -- Like the snakelike paper whistle, the metal tube begins to straighten as the pressure increases inside of it. ** As the tube straightens, the pointer moves around a dial that indicates the pressure typically in psi (14.7 psi= 1 atm). Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.1.1 Diaphragm and Bourdon Bourdon gauge -- Rough indication of pressure Compound gauge: to measure both vacuum and pressure. Differential gauge: to measure the pressure difference. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.1.1 Diaphragm and Bourdon ** Pressure = Force /area -- 1 atm = 0 psig = 14.7 psia ** Vacuum – The removal of gas molecules in a close container to achieve a pressure less than atmosphere. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.1.2 Capacitance Manometers ** A capacitance gauge is simply a diaphragm gauge. ** The deflection of the diaphragm is measured by observing the change in capacitance between it and a fixed counter electrode. ** Measuring absolute pressures. ** The diaphragm provides very low hysteresis, excellent repeatability, remarkably high resolution (1x10-5 of Full Scale), fast response, and the ability to measure extremely low pressures .** A transducer and an electronic sense unit convert the membrane position to a signal linearly proportional to the pressure. Double-sided capacitance manometer: ** 1% difference in dielectric constant will result in a 0.5% error. (Disadvantage) -- Null detector -- Direct reading gauge (Pref < 10-5 Pa) Reference Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.1.2 Capacitance Manometers Single-sided capacitance manometer ** The high vacuum on the reference side is maintained over the life of the manometer by means of an internal chemical getter pump. ** Deflection can be as low as 10-9 cm, motion of parts due to temperature change becomes a large source of error. Ambient temperature at ~ 50ºC. -- Without proper temperature regulation, errors of (1) zero and span coefficient of 5 –50 ppm full scale, and (2) 0.004 –0.04% of reading per degree Celsius.* ** Absolute pressure operated over a large dynamic range. 0.1 torr–10,000 torr. Similar to Fig. 5.4 (P. 85) Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung Piezo-diaphragm vacuum gauges (Micro-Machined Silicon pressure transducers) Pressure-induced strain increases the value of the radial resistors "r", and decreases the value of resistors "t" tangential to the radius. This resistance-change can be as high as 30%. The resistors are hooked up as a Wheatstone bridge. The bridge output is directly proportional to the pressure. http://fieldbus.feld.cvut.cz/en/system/files/files/en/education/courses/xe38ssd/05-Pressure.pdf Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung http://medhycos.mpl.ird.fr/en/data/tec/sensors/keller1bis.pdf 5.2 INDIRECT-READING GAUGES ** By measuring a pressure-dependent property of the gas. ** P > 0.1 Pa in the medium vacuum range region. -- Energy transfer technique, thermal conductivity: Pirani or thermocouple gauges . -- Momentum transfer technique, viscosity: Spinning rotor gauge. ** 0.1 -10-10 Pa in the high to ultrahigh vacuum region, measuring gas density. -- Ionization gauges: Bayard –Alpert and extractor hot cathode gauges, Penning ion gauge, cold cathode gauges. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.1 Thermal Conductivity Gauges ** Thermal conductivity = constant P > 1 torr 0 P ~ 10-3 torr ** Knudsen number, Kn = mean free path / system dimension = λ/ d Viscous flow, Kn < 0.01 Free molecular heat flow P, 0.01 < Kn < 10 ** Used as only rough indicators of vacuum. Convectron gauge A fewλ~ d λ~ d Linear region Thermalcouple, Pirani gauge Thermal energy is transferred by gas bouncing between the heat source and the chamber case. ** To extend the range of a gauge to its lowest possible pressure limit: Heat flow losses ∝ (T24 – T14) + end losses -- End losses dominates when the wire is short. -- Radiation losses increase with wire temperature. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.1 Thermal Conductivity Gauges Pirani gauge A heated wire forms one arm of a Wheatstone bridge. ** A Wheatstone bridge circuit is used to measure the resistance change. ** Nulling: The gauge tube is evacuated to ~ 10-4 Pa and R1is adjusted for balance. ** Compensating tube: To correct for temperature induced changes on nulling. With the compensating (evacuated and sealed) tube, pressure can be measured to 10-3 Pa. ** A low-temperature filament is heated by a constant temperature, current, or voltage. -- Constant temperature: The most sensitive and accurate method. As pressure in the gauge tube increase, more heat is dissipated. Increasing the voltage to move the bridge toward balance. -- Constant voltage or current: The out-of-balance current meter is simply read Chemistry, the pressure. Grace H.calibrated Ho, Departmentto of Applied National University of Kaohsiung 5.2.1 Thermal Conductivity Gauges ** Constant current is delivered to the heated wire. ** Temperature of the filament depends on the rate of heat loss to the surrounding gas. (Thus, its working range is about 1 – 10-3 torr.) ** TC gauge: The temperature is determined by the e.m.f. produced by a Chromel-Alumel thermocouple (K-type) in contact with the filament. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.1 Thermal Conductivity Gauges Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.1 Thermal Conductivity Gauges ** The pressure indicated by the thermal-conductivity gauges depends upon the thermal conductivity of the gas. ** The pressure readings are calibrated by the manufacturer for use with air. ** These gauges can only be expected to be accurate within a factor of two. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 3.3.2 Thermal-Conducting Gauges – Convectron, indirect ** Convectron gauges provide useful pressure measurement over 6 decades from 1 millitorr to 1000 Torr, or from 1 x 10-3 mbar to 1000 mbar. ** This vacuum measurement is accomplished with a single gauge tube. ** The gauge tube contains a temperature compensated heat loss sensor which utilizes conduction cooling to sense pressure at lower pressures. (10-3 to 1 torr) ** At higher pressures, it utilizes convection cooling in which gas molecules are circulated through the gauge tube by gravitational force. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 3.3.2 Thermal-Conducting Gauges – Convectron, indirect ** P < 1 torr, not sensitive to the gas identity. ** P > 1 torr, very sensitive to the gas identity. e. g. Ar at 1000 torr can be read as at “30 torr” by the device! Dangerous!! Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.3 Ionization Gauges – Hot Cathode Gauge ** Usable in the region of molecular flow. 10-3 – 10-10 torr. ** Electron impact ionization, the number of positive ions is proportional to the number density, not the pressure. The current is also depends on the ionization efficiency of the gas in the gauge. (Sensitivity factor) ** Electrons are accelerated through the gas toward a positively biased grid. ** Ions are collected by the ion collector (a fine wire to minimize interception of x-rays). ** The most common gauge is the thermionic or hot-cathode ionization gauge, the most familiar configuration is devised by Bayard and Alpert (B-A type). Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.3 Ionization Gauges – Hot Cathode Gauge Limitation to the low end of the operation range: X-ray ** The X ray limit varies with different gauge designs. ** X rays are produced when the electrons emitted by the cathode impact the grid. ** The B-A type ion gauge means to minimized the x-ray effect. ** When the x-rays strike the collector to produce photoelectrons, the photoelectron currents from the current collectors is detected the same as positive ions arriving at the ion collector. Degassing ** An unbake tubulated gauge should be outgassed. An initial outgassing is typically 15 –20 min. Subsequently outgassing needs only ~ 15 sec. ** Outgassing at P < 10-4 Pa. Ion gauge as a pump ** Ions accelerated to and imbedded in the collector removed from the system. ** Metal evaporated from the filament deposits on the walls to produce a clean, chemically active surface that adsorbs N2, O2, and H2O. Pumping speed is ~ 0.2 liter s-1 for N2 (@ electron-emission current of ~ 10 mA). Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.3 Ionization Gauges – Hot Cathode Gauge “True pressure” = Pressure reading / relative sensitivity Px P( meterreading ) CFx ** Sensitivity in units of microamperes of collector current per unit of pressure per manufacturer’s specified emission current e. g. N2: (100 μA / mTorr)/ 10 mA Filaments: -- Commonly used materials for filaments: tungsten or thoriated iridium. -- More burnout resistant: Coated iridium filaments. Tungsten filaments burn out immediately when exposed to pressures of 0.01 torr or higher . -- More chemical resistant: Reactive tungsten filaments, especially to halogens. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.3 Ionization Gauges – Hot Cathode Gauge “True pressure” = Pressure reading / relative sensitivity Px P( meterreading ) CFx MKS SRS (Standford research systems) Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.3 Ionization Gauges – Hot Cathode Gauge Hot cathode gauge errors: -- X-ray generated photocurrent: fine wire for the ion-collector. -- Electron – stimulated desorption Gas could not adsorb on -- Wall outgassing grids at high temperature. (Why IG operated at 10 mA.) Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung Outdiffusion of H2 from the grid wire. 5.2.3 Ionization Gauges – Cold Cathode (Penning) Gauge Electrons go back and forth through the anode, and finally collide with the anode. S 2 to 10 kV N Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung 5.2.3 Ionization Gauges – Cold Cathode (Penning) Gauge ULVAC Thermionics Cold-cathode ionization gauges ** The cold cathode ionization gauge ionizes the residual gas by an electric discharge. ** A magnetic field forces the electrons on a longer distance in spiral paths before finally colliding with the anode, thereby increasing the ionization probability. ** Cold cathode ionization gauges are rugged and simple. Not mounted immediately adjacent to a hot cathode gauge or residual gas analyzer. ** No X-ray limit, little ESD or thermally induced wall outgassing. ** These gauges are used in the vacuum range from 1 – 10-9 Pa (10-11 torr), therefore, they may have difficulties starting a discharge at very low pressure unless the gauge contains an auxiliary source. (Starting parameter ~ 50 – 500 uPa-s, w/0 Aux.) Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung Semiconductor Requirement The TripleGauge (Inficon) consists of a Bayard-Alpert hot ionization gauge, a Pirani thermal-conductivity gauge, and a miniature alumina capacitance diaphragm gauge. This sensor is capable of covering vacuum measurements from 5×10-10 to 1500 mbar in a single housing. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung Semiconductor Requirement http://www.mksinst.com/docs/UR/900seriesDS.pdf The transducers incorporate MEMS (Micro Electro-Mechanical Systems) based technologies, including MicroPirani™ and Piezo sensors, combined with both Cold Cathode and Mini Ion BA technology resulting in a broad product offering for a wide variety of customer applications. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung Summary of Pressure Gauges Gauge calibration: -- Direct comparison -- Series expansion By government standards institutions and gauge manufacturers. Grace H. Ho, Department of Applied Chemistry, National University of Kaohsiung